Reaction and stratifying container



April 4, 1950 A. T. SWEET 2,502,490

REACTION AND STRATIFYING CONTAINER Filed May 8, 1944 I I-NVENLI'OR ANDREW 7T 5WEET.

ATTORNEY 1936, to 'Svend S. Svensen. "found that-aluminacanbe produced in the form 1 "of 'an" alum pseudomorphs by treating solid alum crystals with ammonia in accordance'with this invention.

Patented Apr. 4, 1950 *U'IT E D --STA I'E-IE'JS PATEN T OF F ICE REACTION AND l STRA TIFYING CONTAINER Andrew T. Sweet, Salt Lake City, Utah, ass'ignor -to "i;he *United States of America as represented by the S'ecretary'of the Interior Application MayFS, 19.44, SerialINo.534,'658

(Granted under the act lo'f'March "3, 1883, .as amended April 30, 1928; 370 0. G. 757) 1 Claim.

iofApril '30, 1928 I (Ch. 460, :45- Stat. L. 46"!) Thistinvention relates .to a method and apparatus :for the production of non-gelatinous "alumina by the treatment of alums With ammonium hydroxide; and provides a-suitable strati- -fying digestion receptacle for the expeditious carrying out of .this'treatment' step.

In the manufacture of alumina by-processes in which alums arezformed as an intermediate prod- 'uct,it is necessary to convert the alumsto. alu- -mina,.'and this operationis usually carried out by treatingthe alumswith'strong aqueous ammonia. i It has been I found that a grainy, non-gelatinous alumin'acan be preparediromalumswhen the -alums,-:either in solid or strongly concentrated solution form, are introduced into a relatively quiescent body of .strongiaqueous ammonia. Heretoforegigreat'difiiculties have been encounteredin this conversion step 'by virtue .of the tendency of the alumina'to precipitate in a gelatinoussstate Which-is=eXtremel difficult to filter, wash, and handle in the subsequent treatment'steps. For

instance, in 'order to produce granular alumina pseudomorphous with the "alum crystals from which itismade, it has heretofore beenlthought necessary tdtreat" the alum crystals'on a complicated belt form apparatus such as is illustrated in U.*S. Patent No."2,036,508, issued on'April 7, It has now'been Through the instrumentality of a novel appagoingtreatment, and includes also a stratifying chemical digestion method adapted to a wide varietyof chemicaltreatment operations. Other objects and advantageswill be-apparentand will appearhereinafter.

'These objects ar accomplished inJaccordance with. this invention which comprises them'ethod,

means, combination and arrangement of parts hereinafter set forth taken in conjunction with l the accompanying drawing.

'fSuit'able apparatus to accomplish the. purposes .-cover2 anda bottom plate .3 which preferably slopes towarda solids outlet-4. Centrally positionedin the coverpZ and depending therefrom is an annular baffle 5 having a closely fittingncover 5. The annular baflle-E-is provided with a plurality-of passageways l for equalizin the yapor pressure inside the bafile .5 and inside the vessel 4. .Near the topbfthe'annular .baffie 5. vare.lo-

oated a solids inlet..8ifor admitting solid feed. material and a vliquid inlet is .forladmitting liquid feed material. A vent idisfllocatednear the top lof the vessel l .for dischargingevolved vapors from the bodybf quiescentliquid.containedin the vessel g I. 1 In ,thecoverltl of r the annular baffle 5-iS;jOHIIl&1Bd EL shaft ll driven througha pulley .l-2 from an suitable sourceof power not shown.

.The shaft ill extends throughout the length of the vesselJ .andlis'similarly journaled in v-abr'acket lv3lnear the base of the ,vessel I. aClosely-adjacentthe bottom -3 of the vessell are a-series-of rake'armsl4 driven by. the shaftll I; and

,adaptedtocscrape sedimentary deposits on the bottom 3 of the vessel-l andvdirect-them toward the solidsoutletA. .Also carried by .thelshaftiil are a series of deflecting vanes'lllzwhich maybe of conical-zorirustroeconical shape mounted colaxially with the shaft below the-annular baffle. 5

and :adapted 1 to cause falling @solids discharged from the upper portion of the vessel 1' to travelran extended path through the quiescent; liquid body toward thev periphery of the .vessel, I Circumferentially l0cated-arou-nd theperipheryof the vesssl I :andsubstantially; below-v the normal liquid level are.aqpluralitybtliquid outlets |6= for withdrawring weakened-.or -.-spent liquid. The-outlets vH5 =-communicate through shortz con duits IT with a toroidal manifold I S-which inturn discharges the weakened liquors through a float controlled valve :19. Thevalve 'l-9-is actuated@automatically by -means ofsarod-zllrand-a bell crankJZI, andthis -bell crank- ZI isshownconnected with a, fioat'22 through a packing gland -23 and-a rack and l pi-nion gear'M.

:Closely above the liquid .-out1ets 1 t6 and overhanging them is showna circumferentialmember .25; projecting v inwardly in "arcuate form from the vessels inner wall. The membere25-shieldsthe liquid outlets lifrom falling-solidsand also serves 3 the multiple function of causing discharged liquids to emanate from the lower portion of the vessel I rather than the upper, and further tends to maintain the liquid contents of the vessel I in a quiescent state.

In operation, the vessel I is filled with strong aqueous ammonia and thereafter the feed ammonia is fed through the liquid inlet 9 preferably in continous manner and the liquid level is maintained constant in the vessel I by virtue of the float 22 actuating the float controlled valve I9. The shaft I I is very slowly rotated at, say 3 to 4 revolutions per minute, in order that the rake arms I4 will cause precipitatin solids to be discharged through the solids discharge 4 at the central part of the vessel bottom 3. Alum to be reacted is introduced into the vessel l by means of the solids inlet 8 into the inner portion of the annular baflle 5 where it immediately contacts the strong aqueous ammonia feed introduced into the inlet 9. As the alum particles settle and leave the. initial reaction zone on the interior of annular baffle 5, they are deflected outwardly toward the periphery of the vessel I by means of the deflecting vanes I5, thus traveling an extended path through the body of quiescent liquid. As the falling particles settle to the bottom 3 of the vessel I they are raked inwardly to the central solids discharge 4 by means of rake arms It with a minimum of disturbance to-the body of quiescent liquid.

Weakened aqueous ammonia or other treatment liquid is withdrawn through the outlets I6 into the manifold I8 and thence discharged for further working up through the float controlled valve I9. The arcuate circumferential shield and baffle 25 causes the discharged liquid to be taken from the zone of minimum concentration because of the fact that weak aqueous ammonia is more dense than strong aqueous ammonia. Therefore, the weakened aqueous ammonia together with accompanying soluble materials such as for example ammonium sulfate produced in the reaction of ammonia with alums, is withdrawn in a simple and expeditious manner.

While the invention has been described with reference to a preferred embodiment thereof, it will b apparent that numerous modifications can be made therein. For example, a concentrated aqueous solution of alum to be converted can be admitted through the inlet 8 instead of a solid feed. 'While the passageways I have been illustrated as a series of drill holes, it is entirely feasible to make the passageways in th form of a slot (not shown) or other opening to equalize the pressure between the inner and outer portions of the annular baiile. While the deflecting vanes I 5 have been shown as conical and frustroconical in shape, they can alternatively be made in any other suitable shape to cause the precipitating solids to travel an extended path through the treatment liquor. While any of the usual materials of construction resistant to aqueous ammonia and alum solutions can be employed, the apparatus is preferably made of ferrous alloys of chromium, nickel and the like which possess an enhanced corrosion resistance. While the invention has been described with reference to operation at atmospheric or moderately increased pressure, it is apparent that the apparatus may be employed at elevated or reduced pressures with equal facility, depending only on the strength of usual materials of construction.

The apparatus in accordance with this invention is especially applicable to continuous opera-' tion and thus possesses numerous advantages over devices which can only be employed for batch operation. For example, the strong aqueous ammonia and the alum feed, either in solid or liquid form, can be continuously fed to the apparatus, the spent ammonia together with dissolved salts is continuously withdrawn through the liquid discharge outlets, and the granular alumina is continuously withdrawn through the solids discharge.

A salient advantage of th apparatus in accordance with this invention where a solid alum feed is employed, is that the alumina produced is in the form of pseudomorphs of the original alum crystals.

If desired, the annular baflle 5 can be extended substantially beyond the cover 2 of the vessel I to allow the alum feed to fall a considerable distance in a vapor atmosphere saturated with ammonia. Another alternative arrangement is to fit the liquid ammonia inlet 9 with a spray nozzle (not shown) and admit feed ammonia in the form of a fine spray in order to admix it with the feed alum being introduced. Suitably, both the liquid inlet 9 and the inlet 8 can be mounted tangential to the annular baiile 5 so as to produce a whirling motion before the feed substances reach the body of quiescent liquid in the vessel.

Many other various changes and modifications will occur to one skilled in the art, and therefore the invention is not limited to the specific details and procedures outlined.

What is claimed is:

In chemical apparatus adapted to the continuous conversion of alum into pseudomorphous alumina by reaction with quiescent aqueous ammonia, the combination with an elongated closed receptacle adapted to hold a quiescent body of liquid therein, of a coaxial annular baflle in the upper portion of said receptacle extending therefrom and below the normal liquid level, said baffie being closed at its upper end and being of small diameter relative to said receptacle, said bafiie having a plurality of radially-extending passageways in said receptacle above said normal liquid level for equalizing vapor pressure in said receptacle and in said baffle, an inlet near the top of said baflle communicatin therewith for introducing alum crystals into said receptacle via said baffle, a second inlet near the top of said baflle communicating therewith for introducing ammonia into said receptacle via said baflle, whereby the introduction of reactants into said receptacle via said baliie does not substantially disturb the quiescent condition of the main liquid body in said receptacle, a centrally-positioned conduit in the bottom of said receptacle for removing and discharging formed alumina therefrom, a rake device for directing solids collecting on the bottom of said receptacle toward said solids outlet, said rake device comprising an axially-disposed rotary shaft carrying near its lower end a plurality of radially-disposed rake arms, and a liquid discharge device near the middle of said elongated receptacle, said liquid discharge device being adapted to the continuous removal of spent ammonia liquor and dissolved byproducts from said receptacle near its midpoint while continuously maintaining a deep strata of strong ammonia precipitating liquor above the zone of liquid removal, said liquid discharge device comprising a plurality of radiallydisposed outlet conduits communicating with said receptacle near its midpoint, a circumferential baflle disposed about the inner periphery of said receptacle overhanging said liquid outlet conduits to prevent withdrawal of falling solids therethrough, a toroidal manifold embracing} said receptacle and communicating with said lilijuld outlet conduits, and a valved outlet on said nian- 5 ifold connected: to? and actuated by a float lnis'aid receptacle to 'maintain a predetermined level in said receptacle.

REFERENCES CITED The following references are of record in file of this patent:

liquid ANDREW 1 SWEET."

" the Number Green Jan. 30, 1945 

